CN102515559A - Method for preparing copper sulfide film with microwave hydrothermal assisted sol-gel method - Google Patents

Method for preparing copper sulfide film with microwave hydrothermal assisted sol-gel method Download PDF

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CN102515559A
CN102515559A CN2011103759104A CN201110375910A CN102515559A CN 102515559 A CN102515559 A CN 102515559A CN 2011103759104 A CN2011103759104 A CN 2011103759104A CN 201110375910 A CN201110375910 A CN 201110375910A CN 102515559 A CN102515559 A CN 102515559A
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sol
deionized water
microwave hydrothermal
reaction
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CN102515559B (en
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黄剑锋
齐慧
张培培
曹丽云
吴建鹏
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Leiling semiconductor equipment (Jiangsu) Co.,Ltd.
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a method for preparing a copper sulfide film with a microwave hydrothermal assisted sol-gel method. The method comprises the following steps of: successively soaking a glass substrate in diluted hydrochloric acid, concentrated sulfuric acid and a mixed solution of hydrogen peroxide and deionized water for activation treatment, adding cupric acetate in ethanol, and then adding triethanolamine to obtain sol A; soaking the activated glass substrate into the sol A, carrying out film coating on the activated glass substrate with an average-rate pulling method, and drying the substrate subjected to film coating; adding thioacetamide or thiourea in the deionized water to obtain a solution D; and transferring the solution D into a microwave hydrothermal reaction kettle, sealing and then putting the reaction kettle in a temperature-pressure double-control microwave hydrothermal reaction instrument and then reacting by selecting a temperature control mode, washing with the deionized water and absolute ethyl alcohol after the reaction is finished, and then drying in vacuum to obtain the copper sulfide film. According to the invention, the copper sulfide film is prepared by using the microwave hydrothermal assisted sol-gel method, thus the advantages of the two methods are sufficiently bonded; and the prepared film is uniform and compact, and is strong in bonding force, high in crystallization degree, low in defect and good in property.

Description

Microwave hydrothermal assisting sol gel method prepares the method for cupric sulfide film
Technical field
The invention belongs to the preparation method of cupric sulfide film, be specifically related to the method that a kind of microwave hydrothermal assisting sol gel method prepares the cupric sulfide film.
Background technology
Owing to the excellent physical chemistry that transient metal sulfide had, receive the very big interest of researcher as having the potential using value in recent years at aspects such as semi-conductor, light-emitting device and superconductions.CuS is very important p N-type semiconductorN, and band-gap energy is 2.0eV.Owing to have excellent conductivity, electricity, optical property, be widely used in fields such as thermopair, spectral filter, solar cell, transmitter and catalysis.
The method for preparing at present sulfide film mainly contains continuous ionic layer absorption reaction method [M.Ali Yildirim, Aytunc Ates; Aykut Astam.Annealing and light effect on structural, optical and electrical properties of CuS, CuZnS and ZnS thin films grown by the SILAR method [J] .Physica.E; 2009,41:1365-1372.], chemical bath method [Qi Liua, Mao Guobing; Ao Jianping.Chemical bath-deposited ZnS thin films:Preparation and characterization [J] .Applied Surface Science, 2008,254:5711-5714.], plasma method [Y.Rodr í guez-Lazcano; H.Mart í nez; Et al.Properties of CuS thin films treated in air plasma [J] .Thin Solid Films, 2009,517:5951-5955.], spray pyrolysis [Cristina Nagcu; Ileana Pop; Et al.Spray pyrolysis deposition of CuS thin films [J] .Materials Letters, 1997,32:73-77.] etc.Yet these methods need special instrument usually, perhaps need strict experiment condition and long reaction times.And owing in the process of synthetic cupric sulfide, a large amount of H is arranged 2S gas generates, as reacts in the system of opening wide and carry out, and then can cause certain pollution to environment inevitably.Therefore, seek a kind of easy handling, environmental friendliness and method with low cost seem rather important.
Summary of the invention
The object of the present invention is to provide a kind of with low costly, simple to operate and eco-friendly microwave hydrothermal assisting sol gel method prepares the method for cupric sulfide film.This method has fully combined sol-gel method technology simple, all even microwave-hydrothermal method rapid heating of plated film, and reaction time is short, and the advantage that percent crystallinity is high prepares the cupric sulfide film.
For achieving the above object, the technical scheme that the present invention adopts is:
1) glass substrate is immersed in the Hydrogen chloride; After using ultrasonic oscillation 30min～60min, clean with distilled water wash, place the mixing solutions of the vitriol oil, ydrogen peroxide 50 and deionized water to carry out activation treatment substrate then; Leave standstill 24-72h; Take out the back and wash respectively, place absolute ethyl alcohol again with zero(ppm) water and absolute ethyl alcohol, subsequent use;
Wherein the volume ratio of the vitriol oil, ydrogen peroxide 50 and deionized water is 1: 1: 1;
2) with analytically pure venus crystals (Cu (CH 3COO) 2H 2O) join in the ethanol, process the clear solution that venus crystals concentration is 0.003mol/L-0.1mol/L, and the trolamine (C of amount of substances such as adding and venus crystals 2H 7NO) as stablizer, place 60 ℃ the water-bath 2-6h that refluxes then, form homogeneous transparent colloidal sol, placing at room temperature afterwards, ageing 6-24h gets Sol A;
3) glass substrate of step 1) being handled dries up with nitrogen, immerses in the Sol A, adopts at the uniform velocity that crystal pulling method carries out plated film to it, and coating times is 1-3 time, and the substrate behind the plated film is designated as B:
4) the B substrate is positioned under the room temperature, dries naturally, put into air dry oven then, continue dry 0.5h, drying temperature is 100-150 ℃, and dried substrate is designated as C;
5) with thioacetamide (C 2H 5NS) or thiocarbamide (SC (NH 2) 2) add in the deionized water, be mixed with the solution D that thioacetamide or thiourea concentration are 0.006mol/L-0.2mol/L;
6) solution D is changed in the microwave hydrothermal reaction kettle; Compactedness is 50%-80%, then the C substrate is vertically put into reaction kettle and vulcanizes, and puts it into after the sealing in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature control mode to react; Temperature of reaction is controlled at 100-150 ℃, and the reaction times is controlled at 10-60min, and reaction naturally cools to room temperature after finishing;
7) substrate is taken out, use deionized water and absolute ethanol washing clean respectively, obtain the cupric sulfide film 40 ℃ of following vacuum-dryings then.
The present invention adopts microwave hydrothermal assisting sol gel method to prepare the cupric sulfide film, has fully combined the advantage of two kinds of methods, and prepared film is even, densification, and bonding force is strong, and percent crystallinity is high, and low defective is functional.This method is with low cost, and is simple to operate, environmentally friendly, is expected to realize scale operation.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the prepared cupric sulfide film of the embodiment of the invention 1.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.
Embodiment 1:
1) glass substrate is immersed in the Hydrogen chloride; After using ultrasonic oscillation 30min, clean with distilled water wash, place the mixing solutions of the vitriol oil, ydrogen peroxide 50 and deionized water to carry out activation treatment substrate then; Leave standstill 24h; Take out the back and wash respectively, place absolute ethyl alcohol again with zero(ppm) water and absolute ethyl alcohol, subsequent use;
Wherein the volume ratio of the vitriol oil, ydrogen peroxide 50 and deionized water is 1: 1: 1;
2) with analytically pure venus crystals (Cu (CH 3COO) 2H 2O) join in the ethanol, process the clear solution that venus crystals concentration is 0.006mol/L, and the trolamine (C of amount of substances such as adding and venus crystals 2H 7NO) as stablizer, place 60 ℃ the water-bath 2h that refluxes then, form homogeneous transparent colloidal sol, placing at room temperature afterwards, ageing 8h gets Sol A;
3) glass substrate of step 1) being handled dries up with nitrogen, immerses in the Sol A, adopts at the uniform velocity that crystal pulling method carries out plated film to it, and coating times is 1 time, and the substrate behind the plated film is designated as B:
4) the B substrate is positioned under the room temperature, dries naturally, put into air dry oven then, continue dry 0.5h, drying temperature is 100 ℃, and dried substrate is designated as C;
5) with thioacetamide (C 2H 5NS) add in the deionized water, be mixed with the solution D that thioacetamide concentration is 0.012mol/L;
6) solution D is changed in the microwave hydrothermal reaction kettle; Compactedness is 80%, then the C substrate is vertically put into reaction kettle and vulcanizes, and puts it into after the sealing in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature control mode to react; Temperature of reaction is controlled at 100 ℃, and the reaction times is controlled at 60min, and reaction naturally cools to room temperature after finishing;
7) substrate is taken out, use deionized water and absolute ethanol washing clean respectively, obtain the cupric sulfide film 40 ℃ of following vacuum-dryings then.
The CuS particle of gained with Japanese D/max2000PCX-x ray diffractometer x analytic sample of science, is found that product is the CuS covellite structure (JCPDS 06-0464) of six side's phases, see Fig. 1.
Embodiment 2:
1) glass substrate is immersed in the Hydrogen chloride; After using ultrasonic oscillation 60min, clean with distilled water wash, place the mixing solutions of the vitriol oil, ydrogen peroxide 50 and deionized water to carry out activation treatment substrate then; Leave standstill 48h; Take out the back and wash respectively, place absolute ethyl alcohol again with zero(ppm) water and absolute ethyl alcohol, subsequent use;
Wherein the volume ratio of the vitriol oil, ydrogen peroxide 50 and deionized water is 1: 1: 1;
2) with analytically pure venus crystals (Cu (CH 3COO) 2H 2O) join in the ethanol, process the clear solution that venus crystals concentration is 0.05mol/L, and the trolamine (C of amount of substances such as adding and venus crystals 2H 7NO) as stablizer, place 60 ℃ the water-bath 3h that refluxes then, form homogeneous transparent colloidal sol, placing at room temperature afterwards, ageing 10h gets Sol A;
3) glass substrate of step 1) being handled dries up with nitrogen, immerses in the Sol A, adopts at the uniform velocity that crystal pulling method carries out plated film to it, and coating times is 3 times, and the substrate behind the plated film is designated as B:
4) the B substrate is positioned under the room temperature, dries naturally, put into air dry oven then, continue dry 0.5h, drying temperature is 150 ℃, and dried substrate is designated as C;
5) with thiocarbamide (SC (NH 2) 2) add in the deionized water, be mixed with the solution D that thiourea concentration is 0.006mol/L;
6) solution D is changed in the microwave hydrothermal reaction kettle; Compactedness is 70%, then the C substrate is vertically put into reaction kettle and vulcanizes, and puts it into after the sealing in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature control mode to react; Temperature of reaction is controlled at 150 ℃, and the reaction times is controlled at 10min, and reaction naturally cools to room temperature after finishing;
7) substrate is taken out, use deionized water and absolute ethanol washing clean respectively, obtain the cupric sulfide film 40 ℃ of following vacuum-dryings then.
Embodiment 3:
1) glass substrate is immersed in the Hydrogen chloride; After using ultrasonic oscillation 50min, clean with distilled water wash, place the mixing solutions of the vitriol oil, ydrogen peroxide 50 and deionized water to carry out activation treatment substrate then; Leave standstill 72h; Take out the back and wash respectively, place absolute ethyl alcohol again with zero(ppm) water and absolute ethyl alcohol, subsequent use;
Wherein the volume ratio of the vitriol oil, ydrogen peroxide 50 and deionized water is 1: 1: 1;
2) with analytically pure venus crystals (Cu (CH 3COO) 2H 2O) join in the ethanol, process the clear solution that venus crystals concentration is 0.003mol/L, and the trolamine (C of amount of substances such as adding and venus crystals 2H 7NO) as stablizer, place 60 ℃ the water-bath 5h that refluxes then, form homogeneous transparent colloidal sol, placing at room temperature afterwards, ageing 24h gets Sol A;
3) glass substrate of step 1) being handled dries up with nitrogen, immerses in the Sol A, adopts at the uniform velocity that crystal pulling method carries out plated film to it, and coating times is 2 times, and the substrate behind the plated film is designated as B:
4) the B substrate is positioned under the room temperature, dries naturally, put into air dry oven then, continue dry 0.5h, drying temperature is 130 ℃, and dried substrate is designated as C;
5) with thioacetamide (C 2H 5NS) add in the deionized water, be mixed with the solution D that thioacetamide concentration is 0.05mol/L;
6) solution D is changed in the microwave hydrothermal reaction kettle; Compactedness is 60%, then the C substrate is vertically put into reaction kettle and vulcanizes, and puts it into after the sealing in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature control mode to react; Temperature of reaction is controlled at 140 ℃, and the reaction times is controlled at 20min, and reaction naturally cools to room temperature after finishing;
7) substrate is taken out, use deionized water and absolute ethanol washing clean respectively, obtain the cupric sulfide film 40 ℃ of following vacuum-dryings then.
Embodiment 4:
1) glass substrate is immersed in the Hydrogen chloride; After using ultrasonic oscillation 40min, clean with distilled water wash, place the mixing solutions of the vitriol oil, ydrogen peroxide 50 and deionized water to carry out activation treatment substrate then; Leave standstill 36h; Take out the back and wash respectively, place absolute ethyl alcohol again with zero(ppm) water and absolute ethyl alcohol, subsequent use;
Wherein the volume ratio of the vitriol oil, ydrogen peroxide 50 and deionized water is 1: 1: 1;
2) with analytically pure venus crystals (Cu (CH 3COO) 2H 2O) join in the ethanol, process the clear solution that venus crystals concentration is 0.08mol/L, and the trolamine (C of amount of substances such as adding and venus crystals 2H 7NO) as stablizer, place 60 ℃ the water-bath 6h that refluxes then, form homogeneous transparent colloidal sol, placing at room temperature afterwards, ageing 15h gets Sol A;
3) glass substrate of step 1) being handled dries up with nitrogen, immerses in the Sol A, adopts at the uniform velocity that crystal pulling method carries out plated film to it, and coating times is 3 times, and the substrate behind the plated film is designated as B:
4) the B substrate is positioned under the room temperature, dries naturally, put into air dry oven then, continue dry 0.5h, drying temperature is 110 ℃, and dried substrate is designated as C;
5) with thiocarbamide (SC (NH 2) 2) add in the deionized water, be mixed with the solution D that thiourea concentration is 0.13mol/L;
6) solution D is changed in the microwave hydrothermal reaction kettle; Compactedness is 50%, then the C substrate is vertically put into reaction kettle and vulcanizes, and puts it into after the sealing in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature control mode to react; Temperature of reaction is controlled at 120 ℃, and the reaction times is controlled at 40min, and reaction naturally cools to room temperature after finishing;
7) substrate is taken out, use deionized water and absolute ethanol washing clean respectively, obtain the cupric sulfide film 40 ℃ of following vacuum-dryings then.
Embodiment 5:
1) glass substrate is immersed in the Hydrogen chloride; After using ultrasonic oscillation 45min, clean with distilled water wash, place the mixing solutions of the vitriol oil, ydrogen peroxide 50 and deionized water to carry out activation treatment substrate then; Leave standstill 60h; Take out the back and wash respectively, place absolute ethyl alcohol again with zero(ppm) water and absolute ethyl alcohol, subsequent use;
Wherein the volume ratio of the vitriol oil, ydrogen peroxide 50 and deionized water is 1: 1: 1;
2) with analytically pure venus crystals (Cu (CH 3COO) 2H 2O) join in the ethanol, process the clear solution that venus crystals concentration is 0.1mol/L, and the trolamine (C of amount of substances such as adding and venus crystals 2H 7NO) as stablizer, place 60 ℃ the water-bath 4h that refluxes then, form homogeneous transparent colloidal sol, placing at room temperature afterwards, ageing 6h gets Sol A;
3) glass substrate of step 1) being handled dries up with nitrogen, immerses in the Sol A, adopts at the uniform velocity that crystal pulling method carries out plated film to it, and coating times is 3 times, and the substrate behind the plated film is designated as B:
4) the B substrate is positioned under the room temperature, dries naturally, put into air dry oven then, continue dry 0.5h, drying temperature is 140 ℃, and dried substrate is designated as C;
5) with thioacetamide (C 2H 5NS) add in the deionized water, be mixed with the solution D that thioacetamide concentration is 0.2mol/L;
6) solution D is changed in the microwave hydrothermal reaction kettle; Compactedness is 80%, then the C substrate is vertically put into reaction kettle and vulcanizes, and puts it into after the sealing in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature control mode to react; Temperature of reaction is controlled at 130 ℃, and the reaction times is controlled at 30min, and reaction naturally cools to room temperature after finishing;
7) substrate is taken out, use deionized water and absolute ethanol washing clean respectively, obtain the cupric sulfide film 40 ℃ of following vacuum-dryings then.

Claims (1)

1. a microwave hydrothermal assisting sol gel method prepares the method for cupric sulfide film, it is characterized in that:
1) glass substrate is immersed in the Hydrogen chloride; After using ultrasonic oscillation 30min～60min, clean with distilled water wash, place the mixing solutions of the vitriol oil, ydrogen peroxide 50 and deionized water to carry out activation treatment substrate then; Leave standstill 24-72h; Take out the back and wash respectively, place absolute ethyl alcohol again with zero(ppm) water and absolute ethyl alcohol, subsequent use;
Wherein the volume ratio of the vitriol oil, ydrogen peroxide 50 and deionized water is 1: 1: 1;
2) with analytically pure venus crystals (Cu (CH 3COO) 2H 2O) join in the ethanol, process the clear solution that venus crystals concentration is 0.003mol/L-0.1mol/L, and the trolamine (C of amount of substances such as adding and venus crystals 2H 7NO) as stablizer, place 60 ℃ the water-bath 2-6h that refluxes then, form homogeneous transparent colloidal sol, placing at room temperature afterwards, ageing 6-24h gets Sol A;
3) glass substrate of step 1) being handled dries up with nitrogen, immerses in the Sol A, adopts at the uniform velocity that crystal pulling method carries out plated film to it, and coating times is 1-3 time, and the substrate behind the plated film is designated as B:
4) the B substrate is positioned under the room temperature, dries naturally, put into air dry oven then, continue dry 0.5h, drying temperature is 100-150 ℃, and dried substrate is designated as C;
5) with thioacetamide (C 2H 5NS) or thiocarbamide (SC (NH 2) 2) add in the deionized water, be mixed with the solution D that thioacetamide or thiourea concentration are 0.006mol/L-0.2mol/L;
6) solution D is changed in the microwave hydrothermal reaction kettle; Compactedness is 50%-80%, then the C substrate is vertically put into reaction kettle and vulcanizes, and puts it into after the sealing in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature control mode to react; Temperature of reaction is controlled at 100-150 ℃, and the reaction times is controlled at 10-60min, and reaction naturally cools to room temperature after finishing;
7) substrate is taken out, use deionized water and absolute ethanol washing clean respectively, obtain the cupric sulfide film 40 ℃ of following vacuum-dryings then.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102863155A (en) * 2012-09-25 2013-01-09 宁波大学 Preparation method of solar thermal shield glass
CN104911567A (en) * 2015-04-24 2015-09-16 中国地质大学（武汉） Method for preparing p-type cuprous oxide thin film material through sol-gel technology
CN107210353A (en) * 2015-02-13 2017-09-26 泽·佩恩 Produce the practical approach of the compound continuous film thermoelectric semiconductor material of aeroge

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CN101698963A (en) * 2009-10-30 2010-04-28 陕西科技大学 Method for preparing CdS film in microwave hydrothermal mode
CN101792173A (en) * 2010-02-08 2010-08-04 许昌学院 Chemical method for synthesizing flaky CuxSy nanocrystalline optoelectronic film controllably at low temperature

Patent Citations (2)

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CN101698963A (en) * 2009-10-30 2010-04-28 陕西科技大学 Method for preparing CdS film in microwave hydrothermal mode
CN101792173A (en) * 2010-02-08 2010-08-04 许昌学院 Chemical method for synthesizing flaky CuxSy nanocrystalline optoelectronic film controllably at low temperature

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102863155A (en) * 2012-09-25 2013-01-09 宁波大学 Preparation method of solar thermal shield glass
CN107210353A (en) * 2015-02-13 2017-09-26 泽·佩恩 Produce the practical approach of the compound continuous film thermoelectric semiconductor material of aeroge
CN104911567A (en) * 2015-04-24 2015-09-16 中国地质大学（武汉） Method for preparing p-type cuprous oxide thin film material through sol-gel technology

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